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A kind of method preparing glufosinate-ammonium acid by glufosinate-ammonium hydrochloride

A technology of glufosinate-ammonium hydrochloride and glufosinate-ammonium, which is applied in the field of glufosinate-ammonium acid, can solve the problems of low processing capacity, unsuitability for industrial production, high cost, etc., achieve high yield and purity, and save water and solvents

Active Publication Date: 2018-12-07
ZHEJIANG RES INST OF CHEM IND CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purity and recovery rate of the glufosinate-ammonium acid that this method makes are all higher, but because the sodium chloride that neutralization produces has only 1.4% solubility in methanol, need to consume a large amount of water and methyl alcohol, in embodiment, In order to obtain 9.02g of 96% glufosinate-ammonium acid, 150mL of methanol and 10mL of water need to be added, the processing capacity is low, and it is not suitable for industrial production

Method used

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  • A kind of method preparing glufosinate-ammonium acid by glufosinate-ammonium hydrochloride
  • A kind of method preparing glufosinate-ammonium acid by glufosinate-ammonium hydrochloride

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Embodiment 1

[0024] 21.75g ​​(0.1mol) of glufosinate-ammonium hydrochloride was added to 50mL of methanol, 6.0g of 28% concentrated ammonia was added at room temperature, stirred overnight at room temperature, filtered, and dried to obtain 17.9g of glufosinate-ammonium with a purity of 98.5%. The recovery rate was 97.4%.

Embodiment 2

[0026] Add 21.75g ​​(0.1mol) of glufosinate-ammonium hydrochloride to 60mL of methanol, add 6.8g of 25% concentrated ammonia water at room temperature, stir at room temperature overnight, then cool down to 5°C for filtration, and dry to obtain 17.5g of grass with a purity of 98.8%. Ammonium phosphonic acid, the recovery rate is 95.5%.

Embodiment 3

[0028] 21.75g ​​(0.1mol) of glufosinate-ammonium hydrochloride was added to 100mL of methanol, 6.8g of 25% concentrated ammonia was added at room temperature, stirred overnight at room temperature, filtered, and dried to obtain 17.0g of glufosinate-ammonium with a purity of 98.7%. The recovery rate was 92.7%.

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Abstract

The invention discloses a method for preparing glufosinate-ammonium acid from glufosinate-ammonium hydrochloride. According to the method, firstly, glufosinate-ammonium hydrochloride is dissolved in alcohol, then ammonia water is added for neutralization, and glufosinate-ammonium acid is separated out. With the method, glufosinate-ammonium acid with the relatively high purity can be obtained in a high-yield manner, and a lot of water and alcohol can be saved, so that the method is suitable for industrial application.

Description

technical field [0001] The invention relates to a method for glufosinate-ammonium acid, in particular to a method for preparing glufosinate-ammonium acid from glufosinate-ammonium hydrochloride. Background technique [0002] Glufosinate-ammonium, the compound (D, L)-2-amino-4-(hydroxyl (methyl) phosphinyl) butyric acid, and its monoammonium salt is the herbicide glufosinate-ammonium (see US4168983). [0003] In the reported methods for producing glufosinate-ammonium acid or glufosinate-ammonium, it is necessary to go through the step of converting glufosinate-ammonium hydrochloride into glufosinate-ammonium acid. For the process of preparing glufosinate-ammonium acid by glufosinate-ammonium hydrochloride, the prior art has the following reports: [0004] Japanese patent JP1979084529 discloses a preparation method of glufosinate-ammonium acid, by first adding 5N sodium hydroxide to glufosinate-ammonium hydrochloride, and then adding ethanol to precipitate glufosinate-ammoniu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30
Inventor 沈方烈王国超郑昀红张晓铭孔小林姚汉清韦伟黄红英
Owner ZHEJIANG RES INST OF CHEM IND CO LTD